Cyclohexanone → HCID 11333556, compound

Participants

Reaction Steps

54 ml (0.5 mole) of cyclohexanone together with 200 ml (1.5 mole) of 1,4-dioxa-8-aza-spiro[4.5]decane III were dissolved in 0.5 l of diethyl ether and stirred for half an hour to form the compound 8-cyclohex-1-enyl-1,4-dioxa-8-aza-spiro[4.5]decane IV. 31 ml of titanium tetrachloride in 0.5 l of n-hexane were then added dropwise at 0° C. within 60 minutes. After the addition the reaction mixture was heated slowly to 20° C. and stirred for a further 24 hours. The precipitate formed was filtered off under suction and discarded. The filtrate was concentrated by evaporation and directly reacted further. The yield was 83 g (0.37 mole, 71%).

Provenance & Evidence